Syncore. Polyvap /Analyst / Reactor

Transcription

1 Syncore Polyvap /Analyst / Reactor en

2 Syncore An efficient, safe and environmentally sound tool for parallel sample processing

3 Syncore comprises three instruments suitable for all aspects of multiple sample processing. Its design concept allows one unit to perform as a parallel evaporator (Polyvap) which can be instantly converted into a parallel concentrator (Analyst) or a parallel reaction station (Reactor). Thus, the field of applications includes fast parallel evaporation of multiple samples, the smooth concentration to pre-defined residual volumes and parallel synthesis. The modular concept Overview page 4, 5 Evaporation to dryness: Polyvap The Polyvap is a unique parallel evaporator which allows fast safe environmentally sound automatic evaporation of samples ranging in volume from 0.5 to 500 ml. Polyvap page 6, 7 Concentration to residual volumes: Analyst Chemical analysis often requires concentration of big volumes to small residual volumes. The Analyst performs this task with a locally cooled appendix. It further provides high recovery rates due to smooth sample processing. Analyst page 8, 9 Parallel synthesis: Reactor The Reactor is designed to give high efficiency and maximum flexibility for parallel and combinatorial synthesis. Great time savings are achieved using optional accessories which optimize the workflow between synthesis and workup stage. Reactor page 10, 11 Accessories page 13

4 Büchi Syncore Line The modular system for evaporat Parallel evaporation: Syncore Polyvap The Platform The Platform is the core component of the three Syncore configurations. It provides basic functions like shaking, heating (150 C) and cooling ( 20 C) with an optional cooling plate. Parallel evaporation of 4, 6, 12, 24, 48 and 96 samples ranging in volume from 500 to 0.5 ml. Each rack has its own PFA-coated alu minium lid with individual vacuum connections. Parallel concentration: Syncore Analyst Concentrate solutions in parallel to a cooled residual volume in formats of 4, 6 and 12. The Flushback Module available in 6 and 12 formats significantly increases recovery rates. Common accessories Recirculating Chiller Deep-Temperature Insulation High-Temperature Insulation Solvent recovery Cooling of the Condenser, Cooling Plate, Receiving Flask, Reflux or Flushback Module is best done with the B-740/14 or MultiStat 40. Low-Temperature Insulation prevents icing of the reaction platform. Increase the efficiency of the evaporation process with an appropriate High-Temperature Insulation Kit. Condense solvents with either a tap water or dry-ice condenser.

5 ion, sample preparation and synthesis 5 A horizontal orbital movement with a maxi mum rotational speed of 600 rpm produces a strong vortex in the sample tube thereby preventing bumping during operation. Temperature profiles can either be preprogrammed in timed stages or can be manually controlled. Parallel Synthesis: Syncore Reactor The Reflux Module available in formats of 24, 48 and 96 affords efficient refluxing. The Inert Gas Module enables operation under inert conditions, manual solvent addition and sampling for the 24 and 48 rack formats. In conjunction with the Vacuum Cover, the reaction mixture is readily concentrated to dryness after synthesis. Perform filtration, washing, parallel solvent dispensing, and liquid-liquid extraction under inert conditions with the Filtration Unit (format 24). Great time saving Applications Vacuum Controller Vacuum Pump A refrigerated receiver reduces the evaporation time by up to 30%. Ideal for evaporation of solvent mixtures without cumbersome breaks. The scope of application in parallel syntheses and sample preparation is shown in several application notes. The programmable Vacuum Controller V-855 can easily cope with complex solvent mixtures and allows automatic distillation. The Vacuum Pump V-700/ V-710 is optimally designed for use with V-855 and Syncore.

6 Evaporation to dryness: Polyvap Efficient parallel evaporation of a wide sample range Parallel evaporation of multiple samples is an essential prerequisite to increase productivity in parallel and multistage synthesis, extraction, quality control and chromatography. The Polyvap solves this problem quickly and safely even with high-boiling solvents. Interchangeable racks make it possible to evaporate samples ranging in volume from 0.5 to 500 ml. Optimal evaporation conditions are automatically adjusted using the optional Vacuum Controller V-855. Syncore Polyvap advantages No cross-contamination High chemical resistance Environmentally sound operation (ISO 14000) Automatic distillation with Vacuum Controller V-855 Evaporation of high-boiling solvents like DMSO and DMF Fully transparent racks in format 4 and 6 Compatibility with the Syncore Reactor and Syncore Analyst Automatic distillation Areas of application Evaporation of chromatography samples Evaporation after parallel extractions Gravimetric analyses in quality control Evaporation after parallel reactions With the help of the vacuum gradient function of the Vacuum Controller V-855 smooth adjustment to the end-vacuum is possible. This function is also ideal for evaporating off solvent mixtures which typically accumulate after chromatography. The settings can be saved in user-defined pressure profiles. Vacuum Controller V

7 Polyvap features 7 Maximum flexibility No cross-contamination High-boiling solvents condenser hot hot hot Exchangeable racks provide maximum flexibility in both sample volume and sample numbers. The racks are available in formats of 4, 6, 12, 24, 48, and 96 samples ranging in volume from 500 ml to 0.5 ml depending on the rack format. Each sample has its own vacuum connection via a vacuum cover. This design principle, together with the use of inert materials such as glass, PFAcoated aluminium and PTFE, prevents cross-contamination. The cover is heatable to 70 C to prevent condensation. Schematic representation of a rack with two tubes individually connected to the heated vacuum cover. The vapor is conducted to the condenser via grooved channels. High-boiling solvents, such as DMSO or DMF, are efficiently evaporated using the High- Temperature Insulation Kit. The kit comprises a rack and cover insulation with Woulff bottle and hose. Performance data Evaporation rates 150 Typical applications Extraction samples Chromatography samples time for evaporation [min] CH 2 Cl 2, 6 x 250 ml Hexane : Acetone 1:1, 12 x 120 ml CH 2 Cl 2 : Hexane 7:3, 12 x 120 ml Rack 6 Rack 12 Rack 24 Rack 96 Conditions: Parallel evaporation using temperature settings of 42 C (rack) and 50 C (vacuum cover). Optimized vacuum gradient for each solvent controlled by the Vacuum Controller V-855. The condenser is cooled with the Chiller B-740/14. Hexane : EtOAc 5:3, 24 x 30 ml MeOH : H 2 O 1:9, 24 x 30 ml MTBE, 96 x 10 ml High-pressure solvent extractions (PSE or ASE**) provide a considerable number of samples within a short period of time. With the PSE, ASE Rack up to 24 samples are evaporated simultaneously sustaining a high sample throughput in routine analysis. In chromatography a large number of samples are pooled in bigger flasks or evaporated individually. The workflow in sample work-up is significantly increased by simultaneous evaporation of multiple samples. Order information for Polyvap specific accessories Positions Working Number of Order-no. Order-no. Order-no. Highvolume [ml] vessels incl. Rack Vacuum Cover Temp. Kit test tubes for PSE, ASE** tubes* for Falcon tubes* test tubes test tubes * Tubes are not included in the rack. ** ASE is a registered trademark of Dionex Corporation.

8 Concentration to residual volumes: Analyst Smooth concentration with high recovery rates Efficient parallel concentration of large sample volumes to pre-defined residual volumes is a cornerstone of virtually every sample preparation technique in environmental analysis and quality control. In addition, smooth evaporation of thermosensitive compounds is crucial in preventing thermal decomposition. The Analyst copes with both tasks by cooling a small appendix at the bottom of the sample vessels. Sample adhesion to the glass wall is prevented by creating a gentle flushing action at the top of the glass wall with partially condensed vapor. Syncore Analyst advantages Smooth concentration to small residual volumes No thermal decomposition High recovery rates No cross-contamination Automatic distillation with Vacuum Controller V-855 Complete solvent recovery Smooth concentration to residual volumes Areas of application Soil analysis Food-processing analysis Quality control Natural product extraction The Analyst sample vessels feature a small appendix at the bottom which is locally cooled by water or a suitable coolant. This stops the evaporation process as the solvent level reaches the top of the cooling zone. Hence, the sample is concentrated in a small, cooled residual volume, thereby preventing thermal decomposition (see scheme on page 9). Except for the water-cooled appendix, the geometry of the Analyst racks are identical with the Polyvap racks. This allows synergetic usage of the corresponding vacuum covers (see p. 7).

9 Analyst features Tubes with appendix Local cooling zones The Flushback Module cooling zone 9 H 2 O out H 2 O in hot cold residual volume hot coolant heating zone residual volume cooling zone H 2 O out H 2 O in The Analyst sample vessels feature an appendix with three different volumes all compatible with the same rack. There are two versions available: with and without graduated level indication. Schematic depiction of the locally cooled appendix of the sample vessel. The solvent evaporates above this cooling zone. The lower temperature in the appendix prevents evaporation under constant vacuum conditions. The Flushback Module is an optional accessory which is placed on top of the rack in formats of 6 or 12. Apart from the cooling zone at the appendix there is an optional Flushback Module available which partially condenses the vapor at the top of the vessels. Thus, the glass wall is continously rinsed resulting in higher recovery rates. Performance data Recovery rates for concentration of polycyclic aromatic compounds (PAH) with the Analyst R-6 (3 ml residual volume) without (left) and with (right) Flushback Module in cyclohexane. recovery rates [%] without Flushback with Flushback Fluoroanthene Conditions: Parallel evaporation using temperature settings of 40 C (rack), 50 C (vacuum cover), 5 C (Flushback Module), 7 C (residual volume). Vacuum gradient from mbar in 30 min. controlled by the Vacuum Controller V-855. Total time for evaporation process: 60 min. Benzo(b)fluoroanthene Benzo(k)fluoroanthene Benzo(g,h,l)perylene Typical applications Right: with Flushback Left: without Flushback The Analyst is designed for applications in which a concentration step is required. This is typically the case in food&feed and environmental analysis, or quality control. Since the sample rests in the cooled appendix the Analyst is also ideal for evaporation of temperature-sensitive compounds. In analysis high recovery rates are essential. For such applications the Flushback Module is strongly recommended. Order information for Analyst specific accessories Positions Working Residual Tubes** Order-no. Order-no. Flushback volume [ml] volume* [ml] no graduation graduated Rack Vacuum Cover Module not available * Other volumes on request ** Tubes are not included in the rack.

10 Parallel Synthesis: Reactor Improve your work-flow in synthesis and work-up Modern parallel synthesis demands a great deal of versatility, efficiency and convenience. This includes features like cooling, refluxing, inert conditions, solvent dispensing, solid-phase chemistry, filtration, liquid-liquid extraction, and evaporation. While performing the reaction and the work-up stage without sample handling, this greatly improves the workflow efficiency. Syncore Reactor advantages Highly versatile and modular Comprises all relevant synthesis and work-up procedures Reaction and subsequent work-up stage in the same vessels without sample handling Copes with solid-phase chemistry including washing, filtration and extraction steps Programmable temperature profiles Reproducible conditions Areas of application Combinatorial chemistry Solid-phase peptide chemistry Heterogenous and homogenous catalysis Process optimization Evaluation of new synthesis methods Application notes The Syncore Reactor has been used for parallel esterification of carboxylic acids, Friedel-Crafts acylation, electrophilic nitration, reductive amination and more. For further information see: > parallel reactors > applications Filtration, liquid dispensing and extraction The Filtration Module is used in conjunction with the rack format 24. The unit not only permits simultaneous filtration of 24 solution- or solid-phase reactions, but also allows simultaneous solvent addition under inert conditions from a standard laboratory dispenser. Washing, filtration, parallel solvent dispensing and liquidliquid extraction are easily performed. The filtrate is N 2 -pressure driven to a receiving vessel, waste or collected to 24 vessels with the Collecting Unit. Both the Filtration and Collecting Unit are manufactured from inert materials and are compatible with virtually all common reagents. Filtration Unit accessories for format 24 Filtration Unit Collection Unit 42940

11 Reactor features Refluxing Inert conditions 11 Low-temperature reactions reflux coolant hot Refluxing is easily carried out by placing the Reflux Module on top of the rack 24, 48 or 96. The module is connected to tap water or a recirculating chiller and cools the top part of every reaction tube. Schematic representation of a test tube heated by the rack and cooled by the Reflux Module. Using a recirculating chiller with a suitable coolant, methanol was heated under reflux at 90 C for two hours with a loss of 0.5 %. The Inert Gas Module accomodates gas in- and outlets for nitrogen or argon connection for air- or moisture-sensitive reactions. In addition, exchangeable septa allow 100 maximal 90 freedom in manual 80 solvent addition or sampling 70 for GC/MS or HPLC analyses 60 under 50 inert conditions. 40 The Cooling Plate in conjunction with a suitable chiller (B-740/14) can cool the platform to 20 C. An Insulation Rack helps prevent icing (format 24, 48 and 96). Cooling Plate Rack Insulation Plate Insulation Performance data Efficient mixing Reproducible conditions Mixing in % The adjustable eccentricity control for the vortex movement ensures complete mixing of the samples for solid and liquid phase chemistry. C Series 1 Series 2 Series 3 Series 4 The temperature is uniform across all positions of the rack. This ensures reproducible reaction conditions with minimal deviation Mixing time in seconds Viscosity: 1 cp 2 cp 3 cp Conditions: Rack 24, round glass tube, filled to depth of 6 cm, eccentricity 4 mm, rotation 460 rpm, viscosity 1, 2 and 4 cp, solids = 2 g silica gel mm Series Series Series Series Deviation from mean value in C. Conditions: Rack 24 with test tubes, 24 x 25 ml water, temperatures measured at the equilibrium state against the intial setting of 80 C for the experiment. Order information for Reactor specific accessories Inert Gas Cover: Vacuum Cover with Inert Gas Module already assembled to one unit Inert Gas Module: Plate can be mounted to the Vacuum Cover instead of the glass plate Positions Working Reaction Order-no. Order-no. Order-no. Inert Order-no. Order-no. Inert volume [ml] vessels Rack Reflux Module Gas Cover Vacuum Cover Gas Module 50 test tubes capped tubes Falcon tubes* ** test tubes test tubes ** ** * Tubes are not included ** On request

12 Order information for complete Syncore instruments Polyvap order matrix 1P 000 Voltage V 50/60 Hz V 50/60 Hz V 50/60 Hz Condenser 0 None Rack type (incl. vacuum cover) 1 Crystal Rack R-4 2 Crystal Rack R-6 3 Rack R-12 4 Standard Rack R-24 5 Falcon Rack R-24 6 Rack R-96 7 Rack R-24 PSE, ASE 8 Rack R-48 S Type S, Standard for chiller or tap water, P+G coated C Type C, Cold trap for dry-ice cooling, P+G coated Round receiving flask, KS 24/20, P+G coated 0 None 1 1 l volume (suggested formats: 24, 96) 2 2 l volume (suggested formats: 4, 6, 12) Analyst order matrix 1A 0 Voltage V 50/60 Hz V 50/60 Hz V 50/60 Hz Condenser 0 None Reactor order matrix 1R 00 S Type S, Standard for chiller or tap water, P+G coated C Type C, Cold trap for dry-ice cooling, P+G coated Round receiving flask, KS 24/20, P+G coated 0 None 2 2 l volume Rack type (incl. Vacuum Cover) 1 Crystal Rack R-4 Analyst 2 Crystal Rack R-6 Analyst 3 Rack R-12 Analyst Voltage V 50/60 Hz V 50/60 Hz V 50/60 Hz Graduated level indication of appendix Y Yes N No Residual volume ml ml ml Condenser 0 None S Type S, Standard for chiller or tap water, P+G coated C Type C, Cold trap for dry-ice cooling, P+G coated Round receiving flask, KS 24/20, P+G coated 0 None 1 1 l volume 2 2 l volume Filtration unit R-24 (instead of Inert Gas Cover) Y Yes N No Rack type (incl. Reflux, Module, Inert Gas Cover) 0 None 4 Standard Rack R-24 5 Falcon Rack R-24 6 Standard Rack R-96 (no Inert Gas Cover) 8 Standard Rack R-48

13 Order information for general Syncore accessories Platform Sample vessel carrier Vessel lid Condensers Refrigerated receiver Basic platform for individual combination to meet personal demands. 230 V V V Carrier for Analyst or Polyvap vessels in formats of 4, 6 and 12. Format R Format R Format R Lid for R-12 and R-6 Analyst and Polyvap tubes. The set comprises 12 or 6 pieces, respectively. Set format Set format Standard condenser (type S) for tap water with rod, clamps, 1 or 2 liter flask. Type S, 1 l flask Type S, 2 l flask Dry-ice condenser (type C) with rod, clamps, 1 or 2 liter flask. Type C, 1 l flask Type C, 2 l flask Receiver with integrated cooling loop used in conjunction with a type S condenser. Refr. receiver Positions 6 Positions 12 Positions 24 Positions 48 Positions 96 Positions Crystal Rack R-4 for working volumes of ml, incl. 4 tubes Crystal Rack R-6 for working volumes of ml, incl. 6 tubes Rack R-12 for working volumes of ml, incl. 12 tubes Rack R-24 for working volumes of 2 30 ml. with 50 tubes for PSE tubes for Falcon tubes Rack R-48 for working volumes of 1 20 ml, incl. 100 test tubes Rack R-96 for working volumes of ml, incl. 100 test tubes Vacuum Cover for all rack formats R-4. Vacuum Cover for all rack formats R-6. Vacuum Cover for all rack formats R-12. Vacuum Cover for all rack formats R-24. Vacuum Cover for rack format R-48. Vacuum Cover for rack format R Optimal operation with other Büchi products Vacuum Controller Vacuum Pump V-700 Vacuum Pump V-710 Recirculating Chiller V-850: Simple Vacuum Controller for manual operation. V-855: Programmable Vacuum Controller with gradient function and automatic distillation (stage probe). V V Probe for AutoDest Chemical resistant PTFE diaphragm pump with a final vacuum of <10 mbar. Recommended configuration with sec. condenser, Woulff bottle and Vacuum Controller V-855. V V-700, V-855, condenser V-700, V-855, cold trap Four head diaphragm pump with a final vacuum of 2 mbar. Recommended configuration with secondary condenser, Woulff bottle and Vacuum Controller. V V-710, V-855, condenser V-710, V-855, cold trap Recirculating chillers for operation with type S condenser, Analyst Rack, Refrigerated Receiver, Reflux- and Flushback Module. B-740, 800 W B-740, 1400 W MultiStat

14 Applications for Syncore The scope of applications in parallel synthesis and sample preparation is shown in many application notes. For further information see: > Parallel reactors > Applications A comprehensive list of optimized evaporation settings for Syncore is online available at: > Applications > Evaporation The Syncore improves the work-flow in multiple sample processing, such as evaporation of chromatography or extractions samples (Büchi B-811, PSE, ASE, soxhlet), sample concentration for GC/MS, HPLC analyses, or parallel synthesis. Technical Data Syncore Platform Dimensions (L x D x H) 480 x 487 x 354 mm Weight 30 kg Power rating 1500 W Temperature range heating plate up to 150 ºC Rotation speed 0 to 600 rpm Eccentricity 0 to 10 mm Programmable temperature 9 steps up to 9 h:59 min programs 20 ºC to +150 ºC 24 V DC Vacuum Cover 120 W, max. 70 C Connection TTL for external on/off signal 24 V DC temperature-controlled valve 24 V DC cooling water valve (0.5 ºC hysteresis) BÜCHI Labortechnik AG Postfach 9230 Flawil 1 Schweiz T F buchi@buchi.com BUCHI Corporation 19 Lukens Drive, Suite 400 New Castle Delaware USA T F Toll Free: us-sales@buchi.com BÜCHI Labortechnik GmbH Postfach Essen Deutschland Freecall T F deutschland@buchi.com BUCHI Hong Kong Ltd Fortress Tower 250 King s Road North Point, Hong Kong China T F china@buchi.com We are represented by more than 100 distribution partners worldwide. Find your local representative at BÜCHI Labortechnik GmbH Branch Office Netherlands Postbus AC Hendrik-Ido-Ambacht The Netherlands T F netherlands@buchi.com BUCHI Shanghai Trading LLC 21/F Shanghai Industrial Investment Building 18 Caoxi Bei Road Shanghai China T F china@buchi.com BÜCHI Italia s.r.l. Centro Direzionale, Milano Fiori Pal. A-4, Strada Assago (MI) Italia T F italia@buchi.com BUCHI UK Ltd 5 Whitegate Business Centre Jardine Way Chadderton Oldham OL9 9QL United Kingdom T F uk@buchi.com BUCHI India Private Ltd. 201, Magnum Opus Shantinagar Industrial Area Vakola, Santacruz (East) Mumbai , India T / 84 / 85 F BUCHI Sarl 5, rue du Pont des Halles Z.A. du Delta Rungis Cedex France T F france@buchi.com BUCHI (Thailand) Ltd., 77/175, Sin Sathon Tower, 39th FL, Unit F Krungthonburi Rd. Klongtonsai, Klongsan Bangkok Thailand T F bacc@buchi.com Nihon BUCHI K.K. 3F IMON Bldg., Ikenohata, Taito-ku, Tokyo Japan T F nihon@buchi.com Quality in your hands en 0807 / Technical Data subject to alterations / Quality System ISO en 0803 / Technical data subject to alterations / Quality Systems ISO 9001